Sodium Hydroxide → 2,3-Dichloro-5-hydroxypyridine

HRID 2302142노트

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HRID 2302142 반응식
[OH-].[Na+].C([O:6][C:7]1[CH:8]=[C:9]([Cl:14])[C:10]([Cl:13])=[N:11][CH:12]=1)(=O)C>O>[Cl:13][C:10]1[C:9]([Cl:14])=[CH:8][C:7]([OH:6])=[CH:12][N:11]=1

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 145952225,6-Dichloropyridin-3-yl acetate

생성물 1

HCID 143916722,3-Dichloro-5-hydroxypyridine

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
0 °C

실험 절차

At 0° C., a solution of 13 g of sodium hydroxide in 80 ml of water was added to 16 g of 5-acetyloxy-2,3-dichloropyridine in 100 ml of ice-water. The mixture was subsequently initially stirred at 0° C. for one hour and then at approximately 20° C. for 17 hours, and the reaction mixture was then washed with 150 ml of ethyl acetate. The mixture was acidified up to a pH of 4-5 by addition of acetic acid and then extracted three times with 100 ml of ethyl acetate each time. The combined organic phases were dried over magnesium sulfate and finally concentrated. Yield: 12.2 g.

후처리

  1. waitat approximately 20° C. for 17 hours
  2. washthe reaction mixture was then washed with 150 ml of ethyl acetate
  3. additionThe mixture was acidified up to a pH of 4-5 by addition of acetic acid
  4. extractionextracted three times with 100 ml of ethyl acetate each time
  5. dry with materialThe combined organic phases were dried over magnesium sulfate
  6. concentrationfinally concentrated

출처 및 근거

ORD 기록
ord-74aee886a2c74b9d862e2dd853fd9b8f
출처 데이터셋
uspto-grants-2002_08
특허 번호
US06432880B1

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